CN106882842A - A kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials - Google Patents
A kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials Download PDFInfo
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- CN106882842A CN106882842A CN201510930681.6A CN201510930681A CN106882842A CN 106882842 A CN106882842 A CN 106882842A CN 201510930681 A CN201510930681 A CN 201510930681A CN 106882842 A CN106882842 A CN 106882842A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to mesoporous petal-shaped ZnCo2O4The synthetic method of meter Sized Materials.At room temperature, by a certain amount of zinc compound, cobalt compound and precipitation from homogeneous solution agent urea are dissolved in a certain amount of solvent, are sufficiently stirred for certain hour, form the solution of stabilization.Mixed solution is carried out into hydro-thermal reaction, room temperature is cooled to afterwards.Products therefrom deionized water or washes of absolute alcohol and centrifugal filtration, in vacuum drying at 50~60 DEG C.The product for obtaining is calcined in air atmosphere, so that it may prepare mesoporous petal-shaped ZnCo2O4Meter Sized Materials.The method preparation process is simple, and material price is cheap, and production can be scaled up completely.
Description
Technical field
The present invention relates to field of material synthesis technology, more particularly to mesoporous petal-shaped ZnCo2O4Nano-solid material
The preparation method of material.
Background technology
ZnCo2O4Material possesses the distinctive property of spinel structure, its excellent electrochemical properties, gas sensing property
Matter and catalytic property etc., be widely used in ceramic material, solid-state gas sensor, different-phase catalyst,
The fields such as sorbing material, ultracapacitor.Recently as the birth and emergence of nanosecond science and technology, and nanometer
The surface that material shows and interfacial effect, small-size effect, quantum size effect, macroscopic quantum tunneling effect
Should with the nano effect such as Dielectric confinement effect, make nano material have the light more superior than block materials, electricity,
Magnetic, heat, sensitivity characteristic and physical mechanical characteristic.The ZnCo of nanostructured2O4Due to the structure of its stabilization
With abundant physical property and cause extensive concern and study.
On ZnCo2O4The preparation method of nano particle have hydrothermal synthesis method, chemical coprecipitation, colloidal sol-
Gel method, self-propagating high-temperature method, ion-exchange etc., the ZnCo that these methods are prepared2O4Nanometer
Although grain uniform particle sizes, good dispersion degree, morphology controllable.But operating process is complicated, influence factor is whard to control,
The ZnCo of pure phase can not be obtained2O4.Mesoporous flower is prepared using homogeneous precipitation method combination hydro-thermal method in the present invention
Flap ZnCo2O4Meter Sized Materials.
Patent No. CN103985858A discloses a kind of lithium ion battery negative material cobalt acid zinc nanometer sheet
Preparation method.It is 1 by mol ratio:2 zinc salt and cobalt salt is in hydrophilic solvent by alkaline reagent in microwave
There are basic hydrolysis in radiation-induced property, generate metal hydroxides or hydrocarbon precursor, then
Low Temperature Heat Treatment is carried out, two-dimensional ultrathin ZnCo is obtained2O4Nanometer sheet, is finally used as lithium ion battery negative material
Material.Preparation process is simple, with low cost, reaction condition is gentle, and whole course of reaction does not need special installation,
The product quality for finally giving is higher, pattern and size uniform.
The content of the invention
It is an object of the invention to provide a kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials.
Compared with other method, the present invention has course of reaction simple, and the reaction time is short, without any complicated behaviour
Make and the advantages of special equipment.The ZnCo of present invention synthesis2O4Microballoon size is more homogeneous, good dispersion,
In petal-shaped and there is meso-hole structure, specific surface area is larger, with good application prospect.
The technical scheme that the present invention takes is：
A kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials, step is as follows：
(1) at room temperature, by a certain amount of zinc compound (zinc sulfate, zinc nitrate, the one kind in zinc chloride),
Cobalt compound (cobaltous sulfate, cobalt nitrate, the one kind in cobalt chloride) and precipitation from homogeneous solution agent urea are dissolved in solvent (water
Or/and ethanol) in, certain hour is sufficiently stirred for, form the solution of stabilization.
(2) mixed solution is transferred in the stainless steel high temperature autoclave of polytetrafluoroethyllining lining,
12~24h is heated at 120~180 DEG C, room temperature is cooled to afterwards.
(3) products therefrom deionized water and absolute ethyl alcohol are respectively washed 3 times, centrifugal filtration, in
It is vacuum dried at 50~60 DEG C.Obtain ZnCo2O4Presoma meter Sized Materials.
(4) dried product heats certain hour under uniform temperature in air atmosphere, prepares mesoporous flower
Flap ZnCo2O4Meter Sized Materials.
The mesoporous petal-shaped ZnCo that above-mentioned experimentation is obtained2O4Meter Sized Materials have homogeneous mesoporous knot
Structure, realizes the purpose of invention.
Brief description of the drawings
Fig. 1 is the mesoporous petal-shaped ZnCo for preparing2O4The XRD piece of meter Sized Materials.
Fig. 2 is the mesoporous petal-shaped ZnCo for preparing2O4The SEM pictures of meter Sized Materials.
Specific embodiment
Further illustrated with reference to specific embodiment.
Embodiment 1：
At room temperature, by 1mmol zinc chloride, 2mmol cobalt chlorides and 12mmol urea are dissolved in 50ml
In water and 30ml ethanol, it is placed on magnetic stirring apparatus, is sufficiently stirred for being allowed to whole dissolvings.Stirring 30min
Afterwards, solution is shifted into a stainless steel high temperature autoclave with polytetrafluoroethyllining lining of 100ml
In, the hydro-thermal reaction 18h at 160 DEG C is placed in Muffle furnace, room temperature is subsequently cooled to, products therefrom is used
Washes of absolute alcohol three times, removes possible remaining impurity, and centrifugal filtration is vacuum dried at 60 DEG C.
By dried product in air atmosphere in calcining 2h at 500 DEG C.Obtain with mesoporous petal-shaped
ZnCo2O4Meter Sized Materials (as shown in Figure 1 and Figure 2).
Embodiment 2：
At room temperature, by 1mmol zinc chloride, 2mmol cobalt chlorides and 12mmol urea are dissolved in 50ml
In water and 30ml ethanol, it is placed on magnetic stirring apparatus, is sufficiently stirred for being allowed to whole dissolvings.Stirring 30min
Afterwards, solution is shifted into a stainless steel high temperature autoclave with polytetrafluoroethyllining lining of 100ml
In, the hydro-thermal reaction 12h at 120 DEG C is placed in Muffle furnace, room temperature is subsequently cooled to, products therefrom is used
Washes of absolute alcohol three times, removes possible remaining impurity, and centrifugal filtration is vacuum dried at 60 DEG C.
By dried product in air atmosphere in calcining 2h at 400 DEG C.Obtain ZnCo2O4Nano-solid
Material.
Embodiment 3：
At room temperature, by 1mmol zinc sulfate, 2mmol cobaltous sulfates and 15mmol urea are dissolved in 50ml
In water and 30ml ethanol, it is placed on magnetic stirring apparatus, is sufficiently stirred for being allowed to whole dissolvings.Stirring 30min
Afterwards, solution is shifted into a stainless steel high temperature autoclave with polytetrafluoroethyllining lining of 100ml
In, the hydro-thermal reaction 24h at 180 DEG C is placed in Muffle furnace, room temperature is subsequently cooled to, products therefrom is used
Washes of absolute alcohol three times, removes possible remaining impurity, and centrifugal filtration is vacuum dried at 60 DEG C.
By dried product in air atmosphere in calcining 30min at 600 DEG C.Obtain ZnCo2O4Nanometer
Solid material.
Embodiment 4：
At room temperature, by 1mmol zinc sulfate, 2mmol cobaltous sulfates and 15mmol urea are dissolved in 80ml
In water, it is placed on magnetic stirring apparatus, is sufficiently stirred for being allowed to whole dissolvings.After stirring 30min, by solution
In one stainless steel high temperature autoclave with polytetrafluoroethyllining lining of 100ml of transfer, horse is placed in
Not in stove at 160 DEG C hydro-thermal reaction 12h, be subsequently cooled to room temperature, products therefrom is clear with absolute ethyl alcohol
Wash three times, remove possible remaining impurity, centrifugal filtration is vacuum dried at 60 DEG C.After drying
Product in air atmosphere in calcining 1h at 500 DEG C.Obtain ZnCo2O4Meter Sized Materials.
Embodiment 5：
At room temperature, by 1mmol zinc nitrates, 2mmol cobalt nitrates and 18mmol urea are dissolved in 80ml
In water, it is placed on magnetic stirring apparatus, is sufficiently stirred for being allowed to whole dissolvings.After stirring 30min, by solution
In one stainless steel high temperature autoclave with polytetrafluoroethyllining lining of 100ml of transfer, horse is placed in
Not in stove at 120 DEG C hydro-thermal reaction 18h, be subsequently cooled to room temperature, products therefrom is clear with absolute ethyl alcohol
Wash three times, remove possible remaining impurity, centrifugal filtration is vacuum dried at 60 DEG C.After drying
Product in air atmosphere in calcining 1h at 400 DEG C.Obtain ZnCo2O4Meter Sized Materials.
Case study on implementation 6：
At room temperature, by 1mmol zinc nitrates, 2mmol cobalt nitrates and 18mmol urea are dissolved in 50ml
In water and 30ml ethanol, it is placed on magnetic stirring apparatus, is sufficiently stirred for being allowed to whole dissolvings.Stirring 30min
Afterwards, by solution shift a stainless steel high temperature autoclave with polytetrafluoroethyllining lining of 50ml in,
The hydro-thermal reaction 12h at 180 DEG C is placed in Muffle furnace, room temperature is subsequently cooled to, products therefrom is with anhydrous
Ethanol is cleaned three times, removes possible remaining impurity, and centrifugal filtration is vacuum dried at 60 DEG C.Will
Dried product is in air atmosphere in calcining 1h at 600 DEG C.Obtain ZnCo2O4Nano-solid material
Material.
Claims (7)
1. a kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials, it is characterised in that：
By zinc compound, cobalt compound and precipitation from homogeneous solution agent are dissolved in solvent, are carried out after being sufficiently stirred for
Hydro-thermal reaction；The product of gained is calcined in air atmosphere, mesoporous petal-shaped is prepared
ZnCo2O4Meter Sized Materials.
2. a kind of mesoporous petal-shaped ZnCo as claimed in claim 12O4The system of meter Sized Materials
Preparation Method, it is characterised in that：Described zinc compound includes：Zinc sulfate, zinc nitrate, chlorination
One or two or more kinds in zinc；Described cobalt compound includes：Cobaltous sulfate, cobalt nitrate, chlorine
Change cobalt in one or two or more kinds；Described precipitation from homogeneous solution agent is：Urea.
3. a kind of mesoporous petal-shaped ZnCo as claimed in claim 12O4The system of meter Sized Materials
Preparation Method, it is characterised in that：Described solvent includes：Water or ethanol.
4. a kind of mesoporous petal-shaped ZnCo as claimed in claim 12O4The system of meter Sized Materials
Preparation Method, it is characterised in that：The method of described hydro-thermal reaction is：Mixed solution is transferred to poly-
Tetrafluoroethene for liner stainless steel high temperature autoclave in heat 12- at 120-180 DEG C
24h, is cooled to room temperature；Products therefrom deionized water and absolute ethyl alcohol are respectively washed 1-6 times, from
The heart is filtered, and in being vacuum dried at 50-60 DEG C, obtains ZnCo2O4Presoma nano-solid material
Material.
5. preparation method as claimed in claim 1, it is characterised in that：Calcining heat：Will calcining
Temperature control is at 400-600 DEG C.
6. the preparation method as described in claim 1 or 5, it is characterised in that：Calcination time：Will
Calcination time is controlled in 30min-2h.
7. preparation method as claimed in claim 1 or 2, it is characterised in that：Zinc compound,
Cobalt compound and the mol ratio of precipitation from homogeneous solution agent are 1:2:12,1:2:15,1:2:18.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108033493A (en) * | 2018-01-22 | 2018-05-15 | 中北大学 | Porous ZnCo2O4The synthetic method of nanometer sheet and pseudo-cubic micro nano structure |
| CN108539183A (en) * | 2018-05-14 | 2018-09-14 | 山东玉皇新能源科技有限公司 | Lithium titanate composite material and preparation method thereof and lithium ion battery negative material and lithium ion battery |
| CN108862403A (en) * | 2018-06-19 | 2018-11-23 | 上海电力学院 | A kind of preparation method and applications of cobalt acid zinc nanometer sheet material |
| CN111239204A (en) * | 2018-11-29 | 2020-06-05 | 有研工程技术研究院有限公司 | Bimetal oxide semiconductor gas-sensitive material and preparation method thereof |
| CN111233049A (en) * | 2020-01-19 | 2020-06-05 | 安徽师范大学 | Sulfur-loaded composite material of zinc cobaltate microspheres with multilayer mesoporous structure and preparation method thereof, lithium-sulfur battery positive electrode and lithium-sulfur battery |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420431A (en) * | 2013-07-31 | 2013-12-04 | 上海理工大学 | Preparation method ofzinc cobaltatenanometer material doped with zinc oxide |
-
2015
- 2015-12-15 CN CN201510930681.6A patent/CN106882842A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420431A (en) * | 2013-07-31 | 2013-12-04 | 上海理工大学 | Preparation method ofzinc cobaltatenanometer material doped with zinc oxide |
Non-Patent Citations (2)
| Title |
|---|
| QINGHONG WANG等: "Facile fabrication and supercapacitive properties of mesoporous zinc cobaltite microspheres", 《JOURNAL OF POWER SOURCES》 * |
| SATYAJIT RATHA等: "Self-assembled flower-like ZnCo2O4 hierarchical superstructures for high capacity supercapacitors", 《RSC ADVANCES》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108033493A (en) * | 2018-01-22 | 2018-05-15 | 中北大学 | Porous ZnCo2O4The synthetic method of nanometer sheet and pseudo-cubic micro nano structure |
| CN108539183A (en) * | 2018-05-14 | 2018-09-14 | 山东玉皇新能源科技有限公司 | Lithium titanate composite material and preparation method thereof and lithium ion battery negative material and lithium ion battery |
| CN108539183B (en) * | 2018-05-14 | 2020-09-25 | 山东玉皇新能源科技有限公司 | Lithium titanate composite material and preparation method thereof, lithium ion battery cathode material and lithium ion battery |
| CN108862403A (en) * | 2018-06-19 | 2018-11-23 | 上海电力学院 | A kind of preparation method and applications of cobalt acid zinc nanometer sheet material |
| CN111239204A (en) * | 2018-11-29 | 2020-06-05 | 有研工程技术研究院有限公司 | Bimetal oxide semiconductor gas-sensitive material and preparation method thereof |
| CN111233049A (en) * | 2020-01-19 | 2020-06-05 | 安徽师范大学 | Sulfur-loaded composite material of zinc cobaltate microspheres with multilayer mesoporous structure and preparation method thereof, lithium-sulfur battery positive electrode and lithium-sulfur battery |
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